In this work, we developed highly porous activated carbon (AC) materials with micro/meso porosity through carbonizing rice husk and treating them with K2CO3. Elemental sulfur was then loaded to the micropores through a solution infiltration method to form rice husk-derived activated carbon (RHAC)aS composite materials.
Trang 1Original Article
Cost-effective porous carbon materials synthesized by carbonizing rice
batteries
Anh-Tuan Lec,d,**
a School of Chemical Engineering, Hanoi University of Science and Technology, Ha Noi, Viet Nam
b Department of Chemical Engineering, National Taiwan University, Taipei 106, Taiwan
c Phenikaa University Nano Institute (PHENA), Phenikaa University, Hanoi 12116, Viet Nam
d Faculty of Materials Science and Engineering, Phenikaa University, Hanoi 12116, Viet Nam
a r t i c l e i n f o
Article history:
Received 18 March 2019
Received in revised form
25 April 2019
Accepted 25 April 2019
Available online 30 April 2019
Keywords:
Rice husk
Cathode material
Carbonization process
Activated carbon
Lithium-sulfur batteries
a b s t r a c t
In this work, we developed highly porous activated carbon (AC) materials with micro/meso porosity through carbonizing rice husk and treating them with K2CO3 Elemental sulfur was then loaded to the micropores through a solution infiltration method to form rice husk-derived activated carbon (RHAC)@S composite materials The as-prepared RHAC@S composites with 0.25 mg cm1and 0.38 mg cm1of sulfur loading were tested as cathodes for lithium-sulfur (Li-S) batteries The 0.25 mg cm1sulfur loaded sample showed an initial discharge capacity of 1080 mA h/g at a 0.1 C rate After 50 cycles of charge/ discharge tests at the current density of 0.2 C, the reversible capacity is maintained at 312 mA h/g The RHAC material delivered a capacity of more than 300 mA h/g at a current density of 1.7 C These results demonstrate that the RHAC porous materials are very promising as cathode materials for the develop-ment of high-performance Li-S batteries
© 2019 The Authors Publishing services by Elsevier B.V on behalf of Vietnam National University, Hanoi This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/)
1 Introduction
The lithium-sulfur (Li-S) battery system is one of the promising
energy storage devices for the next-generation electric power
storage owing to its excellent theoretical energy density of
cathode material due to its low cost, high theoretical capacity
advantages over other batteries, the low electrical conductivities of
employed to improve the conductivity of the cathode, to avert the
Biomass is the most promising carbon precursor for preparing cost-effective porous carbon materials such as activated carbon
well-developed pore structure, a large surface area, and a high
ma-terials (e.g., cherry stone, olive stone, mangrove charcoal, rice husk, peanut shell, cotton wool) have been investigated for obtaining high electric capacities and excellent electrochemical properties
by-products are renewable resources that can be used for energy, chemicals and materials that have shown their applicability in electrochemical energy systems Due to their abundance, low cost, natural regeneration and availability in considerable amounts, these materials are environmentally friendly renewable resources
accommo-date the current mass volume expansion during cycling It is
* Corresponding author.
** Corresponding author Phenikaa University Nano Institute (PHENA), Phenikaa
University, Hanoi 12116, Viet Nam.
E-mail addresses: tung.maithanh@hust.edu.vn (T.-T Mai), tuan.leanh@
phenikaa-uni.edu.vn (A.-T Le).
Peer review under responsibility of Vietnam National University, Hanoi.
Journal of Science: Advanced Materials and Devices
https://doi.org/10.1016/j.jsamd.2019.04.009
2468-2179/© 2019 The Authors Publishing services by Elsevier B.V on behalf of Vietnam National University, Hanoi This is an open access article under the CC BY license
Journal of Science: Advanced Materials and Devices 4 (2019) 223e229
Trang 2the pore diameter distribution, the pore volume, and the sulfur
filling are the critical factors for optimizing battery performances
promising carbon precursors for producing low-cost activated
million tons of rice husk biomass is generated globally in 2012 The
and lignin, which yield activated carbon when pyrolyzed under an
mate-rials, derived from RH, were developed using different techniques
Their potential application in energy storage systems was also
and activated it by NaOH The optimized AC material with a high
structure through carbonizing the RH and activating it with
activated carbon in order to demonstrate a high potential for
as-prepared rice-husk-derived activated carbon (RHAC) materials
materials for Li-S battery applications we controlled the chemical
an activation agent due to its high activating capability, its
re-striction of the formation of tar and its relatively low cost
In this study, we present an alternative way for synthesizing
micro/mesoporous activated carbon with low cost which is easy to
scale up for Li-S batteries The porous RHAC materials were
The RHAC@S composites were synthesized by the method of
melting diffusion The synergetic effect of the meso/microporosity
and structure on the electrochemical performance of the RHAC@S
cathode was investigated in detail
2 Experimental
2.1 Preparation of activated carbon from rice husk
The rice husks used as carbon precursors for the preparation of
activated carbon were collected from Thai Binh province, Vietnam
deionized (DI) water several times to remove impurities and was
removal of silica from the rice husk, the sample was subjected to
atmo-sphere After cooling, the obtained samplea were washed with DI
2.2 Preparation of activated carbon from rice husk/sulfur composites (RHAC@S)
The RHAC and Sulfur (S) composites were prepared by using a conventional melting diffusion strategy Samples with different
temperature, RHAC@S composites were obtained with sulfur
2.3 Characterizations
calculated using the Brunauer-Emmett-Teller (BET) method X-ray diffraction (XRD) was carried out with a D Max/2000 PC (Rigaku, Ltd) The surface morphologies of the composites were investigated with a scanning electron microscope (SEM, Hitachi, S4700) equip-ped with energy dispersive spectroscopy (EDS, OXFORD 7593-H) 2.4 Electrochemical measurement
Coin cells of the 2032-type were used to study the electrochemical performance of the RHAC@S cathodes The cathodes for the battery test cells were prepared by dispersion/ dissolution of a mixture of the active material RHAC@S (60 wt%),
%) in N-methyl-2-pyrrolidene and super P carbon black (con-ducting agent-Timcal) (20 wt%) Next, the cathode slurry was
nitrogen atmospheric and roll-pressed before use Lithium foil (Li) and Celgard 2400 sheets were used as the anode and separator,
used as the electrolyte
Studies of the charge and discharge properties of the cathodes were performed on a cell life test system (PNE solution, KOREA) These properties were measured at different current densities in the
(CV) experiments were conducted using an electrochemical analyzer (America, Bio-logic, VSP) on the same instrument in the voltage
spectra were recorded by applying an AC voltage of 5 mV amplitude
values were calculated according to the mass of sulfur Our electro-chemical tests were performed at room temperature
3 Results and discussion 3.1 Microstructure and characterization of RHAC
Firstly, we examined the microstructure and characterization of
of the RHAC-600 and RHAC-800 samples The main diffraction peaks
& activated carbon from rice husk.
T.-T Mai et al / Journal of Science: Advanced Materials and Devices 4 (2019) 223e229 224
Trang 3of graphitic carbon could hardly be recognized in the pattern of the
RHAC samples, suggesting a generally amorphous nature for the
crystal planes of graphite, and the broad peaks indicate the
XRD patterns of RHAC-600 and RHAC-800, demonstrating that no
graphitization occurred during the thermal treatment process To
further examine the formation of activated carbon, we measured
Raman spectra and BET surface areas of the 600 and
RHAC-800 samples as shown in the supporting information (SI) The
Raman spectrum of the RHAC exhibits characteristic G- and
carbo-naceous structure of the activated carbon, while the G band
both D- and G-bands are changed in the spectra of the RHAC-600
and RHAC-800 samples, indicating that the carbon matrix changes
due to the increased carbonization temperature The intensity ratio,
on cluster sizes and distributions In our present case, the intensity
indicated a high percentage of structural defects in the RHAC
was noted that higher carbonization temperature would lead to the
production of more micro/mesopores and, therefore, result in
be observed, the isotherms typically display three steps with
the increase in relative pressure and indicate the existence of a
pore size range from micropores to macropores The Nitrogen
the adsorption mechanism and porous structure of the
0.05, is a steeply increasing region which represents the
conden-sation in small micro/mesopores Then, with a relative increase in
pressure, the adsorption amount slowly increases without any
micro/mesopores Finally, near the saturation pressure of nitrogen,
the adsorption amount increases abruptly because of active capil-lary condensation The density functional theory (DFT) model was used to calculate the pore size distributions of the samples The
amount of micro-porosity The RHAC sample exhibites hierarchical
this adsorption isotherm type, these RHAC samples are predomi-nantly of a mesoporous and microporous structure The materials with high surface area and relatively large mesopore sizes are attractive materials for lithium-sulfur batteries With the obtained excellent surface areas, the RHAC-800 sample was selected for sulfur loading for the next measurement
3.2 Microstructure and characterization of RHAC@S
gasi-fication of volatiles upon activation The pores are of different sizes and different shapes However, the particles displayed
sur-faces of the activated carbons are full of cavities, are quite irregular as
slit-shaped micro/mesopores It has been noted that the cavities result
sample, it can be seen that the peak of silicon did not appear which can surmise that the generation of pores is due to the removal of
disap-pear and some macropores change into mesopores in the RHAC@S
employed to detect the chemical composition of the RHAC-800 and
car-bon (C), oxygen (O) in RHAC-800 samples and carcar-bon (C) and sulfur
distributions
peaks of graphitic carbon are not observed in the patterns of the
the carbon material The characteristic peaks of element sulfur can
of crystalline sulfur in the XRD pattern increase with increasing
sulfur into the RHAC samples as well, in good agreement with the EDS analysis
type I isothermal plots with hysteresis loops that indicate the
average pore width of 3.2 nm The high surface area and relatively large mesopore sizes are attractive because they allow the electrolyte
Sulfur
RHAC_800
RHAC_600
2 theta (deg.)
(a) (b)
Fig 2 X-ray diffraction patterns of (a) RHAC-600 and (b) RHAC-800 samples.
T.-T Mai et al / Journal of Science: Advanced Materials and Devices 4 (2019) 223e229 225
Trang 43.3 Electrochemical characterizations of RHAC@S cathode material
composites as cathode material for Li-S batteries has systematically
perform the electrochemical reaction mechanism The pair of sharp redox peaks indicate that during charge/discharge the
narrow oxidation peak around 2.5 V is mainly attributed to the
com-posite electrodes with different loaded sulfur content, shown in
Fig 7, are in good agreement with the C-V curves All the discharge
(a)
(c)
(b)
0.25 (mg cm -2
)
0.38 (mg cm -2
)
Sulfur
2theta (deg.)
Fig 4 XRD patterns of (a) pure S and RHAC 800 @S composites with sulfur loading
content of (b) 0.25 mg cm2and (c) 0.38 mg cm2.
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
0
50
100
150
200
250
300
350
400
3 /g)
Relative Pressure (P/P
o)
RHAC @ S RHAC
adsorptionedesorption isotherms of RHAC-800 and RHAC
1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0 3.2 -1.5
-1.0 -0.5 0.0 0.5 1.0 1.5 2.0 2.5
Fig 6 Cyclic voltammetry curves of RHAC 800 @S electrode with 0.25 mg cm2of sulfur
1 in a voltage range 1.5e3.0 V.
Fig 3 SEM images and EDS elemental mapping of (a,b,c) RHAC-800 and (a’,b’,c’) RHAC 800 @S samples.
T.-T Mai et al / Journal of Science: Advanced Materials and Devices 4 (2019) 223e229 226
Trang 5voltage plateau regions, corresponding to the multistep reduction
reaction of sulfur during the discharge process Moreover, the
up-per plateau at approximately 2.3 V is caused by the conversion of
indi-cating a high utilization of active sulfur This could be due to the
the excellent electrolyte adsorption capability of highly porous
activated carbon materials After the initial loss of capacity
result-ing from the decomposition of the electrolyte and the formation of
a solid electrolyte interphase (SEI) layer, the capacities at 0.1 C
current rate decrease to 900 and 819 mA h/g for the cathodes with
all the samples at a rate of 0.2 C between 1.8 and 2.8 V of the
decays drastically upon cycling for all samples For cells with
rate, the capacity stabilizes at 750 mA h/g and retains at 358 mA h/
g after 50 cycles a 47.73% capacity retention The capacity of cells
680 mA h/g after activating the process and retains at 312 mA h/g after 50 cycles with 45.88% capacity retained The fast capacity
expansion and re-distribution of the active-sulfur during the
higher discharge capacities in each cycle because of the high electron conductivities of the electrodes provided by the carbon, which may promote the electrochemical reactions of sulfur with
with capacities of 1041, 650, 486, 395 and 305 mA h/g at current densities of 0.1, 0.2, 0.5, 0.9 and 1.7C, respectively For the cells
0.1C, 570 mA h/g at 0.2C, 412 mA h/g at 0.5C, 317 mA h/g at 0.9C, and 210 mA h/g at 1.7C The excellent rate performance indicates
different rates
real axis is composed of the ionic resistance of the electrolyte, the intrinsic strength of the active materials and the contact resistance
of the interface between the electrodes and current collectors As
depressed semicircle in the high-frequency region and of a short inclined line (Warburg impedance) in the low-frequency region
originating from the interactions between the electrode and elec-trolyte solvent, result in the semicircle in the high-frequency
on the electrode surface in a non-aqueous organic solution can
Fig 7 Initial charge-discharge profiles of RHAC 800 @S at a current density of
167.5 mA h/g in a voltage range 1.8e2.8 V.
0
100
200
300
400
500
600
700
800
-1 )
Cycle number
0.38 (mg cm-2
) 0.25 (mg cm-2
)
Fig 8 Cycling performance of the RHAC 800 @S samples at 335 mA h/g in a voltage
range of 1.8e2.8 V.
1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 0
200 400 600 800 1000 1200
0.9C
1.7C 0.5C
0.2C 0.1C
-1 )
Cycle number
0.25 (mg cm-2
) 0.38 (mg cm-2)
Fig 9 Rate capability performance of RHAC 800 @S samples at different C-rates in a voltage range of 1.8e2.8 V.
T.-T Mai et al / Journal of Science: Advanced Materials and Devices 4 (2019) 223e229 227
Trang 6impedance (Wo) is related to the lithium ion diffusion within the
With the rise of sulfur loading, the polarization becomes more
considerable, indicating slower dynamics and increasing electrode
po-larization and charge transfer resistant is smallest
4 Conclusion
We developed a hierarchically micro/mesoporous structure of
activated carbon from rice husk via a simple carbonization process
sample showed an amorphous nature with a high surface area
when evaluated as a cathode material for lithium-sulfur batteries,
exhibite a high discharge capacity of 1080 mA h/g, as well as an
excellent cycle stability and a high rate capability We believe that
our results will open new avenues for the development of
high-performance Li-S batteries at using cost-effective porous carbon
materials
Acknowledgements
The authors are grateful to Project NDT.19.TW/16 (Ministry of
Science and Technology, Vietnam) and project 15/FIRST/1.a/HUST
and MOST 105-E002-012-MY12 (Ministry of Science and
Appendix A Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.jsamd.2019.04.009
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0
30
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Z-Z' (ohm)
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) 0.25 (mg cm-2
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